CN114956605B - Method for recycling quartz tube - Google Patents

Method for recycling quartz tube Download PDF

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Publication number
CN114956605B
CN114956605B CN202210754496.6A CN202210754496A CN114956605B CN 114956605 B CN114956605 B CN 114956605B CN 202210754496 A CN202210754496 A CN 202210754496A CN 114956605 B CN114956605 B CN 114956605B
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quartz tube
quartz
pure water
recycling
soaking
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CN114956605A (en
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吕新杨
何世杰
王骏闻
郭晨光
尹士平
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Anhui Guangzhi Technology Co Ltd
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Anhui Guangzhi Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0095Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous glass
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/14Other methods of shaping glass by gas- or vapour- phase reaction processes
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0075Cleaning of glass
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0085Drying; Dehydroxylation
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/32Non-oxide glass compositions, e.g. binary or ternary halides, sulfides or nitrides of germanium, selenium or tellurium
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)
  • Glass Melting And Manufacturing (AREA)

Abstract

The application discloses a recycling method of a quartz tube, which comprises the following steps: cutting off a quartz tube along a vapor transmission tube, and treating a fracture; step two, placing the treated quartz tube in sodium hydroxide solution for soaking; taking out the quartz tube after the soaking is finished, using pure water to wash out alkali liquor attached to the surface of the quartz tube, transferring the alkali liquor into aqua regia for soaking, then using the pure water to spray the outer wall of the quartz tube, then pouring two thirds of pure water into the quartz tube, shaking the bottle body for 8-10 times, then draining washing water in the bottle, and repeatedly cleaning until residual water at the inner side of the bottle forms a film-shaped water film to uniformly flow down; step four, using a pure water spray pipe body, drying, and taking along with use in the use process; and fifthly, the quartz tube can be used for melting the chalcogenide glass bar stock by using high-purity raw materials. The method disclosed by the invention realizes recycling of the quartz tube for distilling and purifying the chalcogenide glass leftover materials, and greatly reduces the cost of distilling and purifying the chalcogenide glass leftover materials.

Description

Method for recycling quartz tube
Technical Field
The invention relates to the field of recycling, in particular to a recycling method of a quartz tube.
Background
The chalcogenide glass is a medium-long wave infrared optical material with excellent performance, and is widely applied to the production fields of infrared lenses, thermal imaging lenses and the like. But in chalcogenide glasses such as H 2 O, hydroxyl and other impurities can seriously affect the infrared transmittance of chalcogenide glass, so that lens materials with strict requirements on transmittance and transmittance wave band generally need to be purified in the preparation process of raw materials with relatively low purity. Due to chalcogenides in large partThe method has the characteristics of high saturated vapor pressure and easy sublimation and gasification, so that the chalcogenide glass can be purified by utilizing the characteristic of large difference between the saturated vapor pressure of the chalcogenide compound and the saturated vapor pressure of impurities and oxides. In addition, the processing leftover materials and defective products with corresponding proportions can be produced in the processes of cold processing and mould pressing processing of the lens materials, and the leftover materials can be purified and recovered by adopting a distillation purification method, so that the resources are effectively saved, and the production cost is reduced.
The method is characterized in that an H-shaped quartz ampoule bottle is generally used for carrying out distillation purification on chalcogenide glass raw materials and leftover materials, raw material filling is carried out on one side of the H-shaped quartz tube, the distillation purification on the raw materials or the leftover materials is realized by controlling the temperature difference between the two tubes, and the chalcogen element has higher vapor pressure at a relatively low temperature, so that the high-temperature process of the quartz ampoule bottle during distillation is relatively mild. Therefore, after distillation and purification are completed, the Cheng Liaoguan of the original H-shaped quartz tube still has excellent thermal and mechanical properties, and if the recycling of the quartz tube on the material containing side can be realized, the use of the quartz tube in the preparation process of chalcogenide glass can be reduced, so that the purposes of resource saving and cost saving are achieved.
Disclosure of Invention
In view of the problems existing in the prior art, an object of the present disclosure is to provide a method for recycling a quartz tube.
In order to achieve the above object, the present disclosure provides a recycling method of a quartz tube, comprising the steps of: cutting off a quartz tube along a vapor transmission tube, and treating a fracture; step two, placing the treated quartz tube in sodium hydroxide solution for soaking, and keeping the temperature of alkali liquor at 80-100 ℃ in the soaking process; taking out the quartz tube after the soaking is finished, using pure water to wash out alkali liquor attached to the surface of the quartz tube, transferring the alkali liquor to aqua regia for soaking for 1-2 h, then using the pure water to spray the outer wall of the quartz tube, then pouring two thirds of pure water into the quartz tube, shaking the bottle body for 8-10 times, then draining washing water in the bottle, and repeatedly cleaning for 3-5 times until residual water at the inner side of the bottle forms a film-shaped water film to uniformly flow down; step four, using the pure water spray pipe body for 2-3 min, drying, and taking the pure water spray pipe body as required in the use process; and fifthly, the quartz tube can be used for melting the chalcogenide glass bar stock by using high-purity raw materials.
In some embodiments, in step one, the means for severing the quartz tube may be a water cut grinding wheel.
In some embodiments, in step one, the operation of handling the fracture is: the fracture is washed and wiped clean, and the cutting fracture is slightly burned by oxyhydrogen flame to remove burrs and cutting cracks at the fracture.
In some embodiments, in step two, the sodium hydroxide is at a mass concentration of 10%.
In some embodiments, in step two, the soaking time is 2-3 hours.
In some embodiments, in step three, the quartz tube outer wall is sprayed with pure water for 3-5 minutes.
In some embodiments, in step four, the drying temperature is maintained at 110-120 ℃.
In some embodiments, in step four, the drying time is maintained at 3-5 hours.
In some embodiments, in step five, the method for melting the chalcogenide glass bar stock from the high purity raw material by using the quartz tube comprises the following steps:
transferring the dried quartz tube into a glove box for raw material filling, placing a charging hopper into a charging port, then carrying out batching and charging operations according to the elemental composition and the stoichiometric ratio of the chalcogenide glass, installing a vacuum quick connector on the charging port of the quartz tube after batching and charging are completed, transferring the quartz tube onto a vacuum unit for vacuumizing treatment, and when the pressure in the tube is lower than 10 -3 And (3) after Pa, sealing and sealing the quartz tube by using oxyhydrogen flame.
The beneficial effects of the present disclosure are as follows:
the method disclosed by the invention realizes recycling of the quartz tube for distilling and purifying the chalcogenide glass leftover materials, and greatly reduces the cost of distilling and purifying the chalcogenide glass leftover materials.
Detailed Description
The method for recycling the quartz tube according to the present application will be described in detail below.
The application discloses a recycling method of a quartz tube, which comprises the following steps: cutting off a quartz tube along a vapor transmission tube, and treating a fracture; step two, placing the treated quartz tube in sodium hydroxide solution for soaking, and keeping the temperature of alkali liquor at 80-100 ℃ in the soaking process; taking out the quartz tube after the soaking is finished, using pure water to wash out alkali liquor attached to the surface of the quartz tube, transferring the alkali liquor to aqua regia for soaking for 1-2 h, then using the pure water to spray the outer wall of the quartz tube, then pouring two thirds of pure water into the quartz tube, shaking the bottle body for 8-10 times, then draining washing water in the bottle, and repeatedly cleaning for 3-5 times until residual water at the inner side of the bottle forms a film-shaped water film to uniformly flow down; step four, using the pure water spray pipe body for 2-3 min, drying, and taking the pure water spray pipe body as required in the use process; and fifthly, the quartz tube can be used for melting the chalcogenide glass bar stock by using high-purity raw materials.
In some embodiments, in step one, the means for severing the quartz tube may be a water cut grinding wheel.
In some embodiments, in step one, the operation of handling the fracture is: the fracture is washed and wiped clean, and the cutting fracture is slightly burned by oxyhydrogen flame to remove burrs and cutting cracks at the fracture.
In some embodiments, in step two, the sodium hydroxide is at a mass concentration of 10%.
In some embodiments, in step two, the soaking time is 2-3 hours. Too short soaking time can easily cause insufficient cleaning of Cheng Liaoguan, and residues still adhere to the wall of the quartz tube; too long soaking time can reduce cleaning efficiency.
In the third step, the quartz tube is soaked by aqua regia to remove trace alkali residues and dirt attached to the inner wall and the outer wall of the quartz tube.
In some embodiments, in step three, the quartz tube outer wall is sprayed with pure water for 3-5 minutes.
In some embodiments, in step four, the drying temperature is maintained at 110-120 ℃.
In some embodiments, in step four, the drying time is maintained at 3-5 hours.
In some embodiments, in step five, the method for melting the chalcogenide glass bar stock from the high purity raw material by using the quartz tube comprises the following steps:
transferring the dried quartz tube into a glove box for raw material filling, placing a charging hopper into a charging port, then carrying out batching and charging operations according to the elemental composition and the stoichiometric ratio of the chalcogenide glass, installing a vacuum quick connector on the charging port of the quartz tube after batching and charging are completed, transferring the quartz tube onto a vacuum unit for vacuumizing treatment, and when the pressure in the tube is lower than 10 -3 And (3) after Pa, sealing and sealing the quartz tube by using oxyhydrogen flame.
[ test ]
Example 1
The component is As 40 Se 60 The sulfur-based glass cold-processing leftover materials are purified to form an H-shaped quartz tube.
Cutting off a residual steam transmission pipe connected with a material containing pipe of an original H-shaped quartz pipe at a position with a joint of about 100mm, cleaning dirt at a fracture, and burning the fracture by using oxyhydrogen flame to remove defects such as burrs at the fracture;
step two, placing the treated quartz tube in 10% sodium hydroxide solution for soaking for 2 hours, and keeping the temperature of the alkali liquor at 80 ℃ in the soaking process;
taking out the quartz tube after the soaking is finished, draining alkali liquor in the tube, using pure water to wash the alkali liquor attached to the surface of the quartz tube, transferring the alkali liquor into aqua regia for soaking for 1h, then using the pure water to spray the outer wall of the quartz tube, then filling two thirds of pure water into the quartz tube, shaking the bottle body for 8 times, draining washing water in the bottle, and repeatedly cleaning for 3 times until residual water at the inner side of the bottle forms a film-shaped water film to uniformly flow down;
step four, using a pure water spray pipe body for 2min, wherein the drying temperature is 120 ℃, the drying time is 3h, and the pure water spray pipe body is taken along with use in the use process;
transferring the dried quartz tube into a glove box for loading operation, and raw materialsFor high-purity selenium and high-purity arsenic with purity of 5N, accurately weighing 581.203g of high-purity arsenic and 918.797g of high-purity selenium by using an electronic balance, sequentially filling two raw materials into a quartz tube along a filling port by using a funnel, assembling a vacuum quick interface at a tube port after filling, transferring the quartz tube out of a glove box, quickly connecting a vacuum unit pipeline for evacuation treatment, keeping the quartz tube in a heating state during evacuation, and keeping the heating temperature at 120 ℃ until the pressure in the quartz tube is evacuated to 10 DEG C -3 After Pa or less, the quartz tube was sealed with oxyhydrogen flame.
Transferring the sealed quartz tube into a swinging furnace for melting homogenization
After the melting is finished, using compressed air as a quenching medium to quench and shape the glass liquid, wherein the quenching air pressure is 0.3MPa, transferring the quartz tube to an annealing furnace to anneal after the glass liquid is hardened and shaped,
after the annealing is finished, the quartz tube is broken, the glass bar stock is taken out, corresponding detection is carried out on the bar stock, and the detection results are shown in the following table:
TABLE 1 As prepared by the same batch of recycled quartz tube 40 Se 60 Bar stock test results
Three quartz tubes processed in the same batch are used for preparing chalcogenide glass bars with the components of As40Se60, and the obtained bars are respectively detected according to national standard test standards, and the results show that: the fringe degree of the three bars is A level, the impurity degree is 1 level, and the transmittance of the three bars corresponding to different incident wavelengths and wave bands is shown in the table above.
Example 2
The component is Ge 28 Sb 12 Se 60 The sulfur-based glass cold-processing leftover materials are purified to form an H-shaped quartz tube.
Cutting off a residual steam transmission pipe connected with a material containing pipe of an original H-shaped quartz pipe at a position with a joint of about 80mm, cleaning dirt at a fracture, and burning the fracture by using oxyhydrogen flame to remove defects such as burrs at the fracture;
step two, placing the treated quartz tube in 10% sodium hydroxide solution for soaking for 2 hours, and keeping the temperature of the alkali liquor at 80 ℃ in the soaking process;
taking out the quartz tube after the soaking is finished, draining alkali liquor in the tube, using pure water to wash the alkali liquor attached to the surface of the quartz tube, transferring the alkali liquor into aqua regia for soaking for 1h, then using the pure water to spray the outer wall of the quartz tube, then filling two thirds of pure water into the quartz tube, shaking the bottle body for 8 times, draining washing water in the bottle, and repeatedly cleaning for 3 times until residual water at the inner side of the bottle forms a film-shaped water film to uniformly flow down;
step four, using a pure water spray pipe body for 2min, wherein the drying temperature is 120 ℃, the drying time is 3h, and the pure water spray pipe body is taken along with use in the use process;
transferring the dried quartz tube into a glove box for loading operation, wherein raw materials are high-purity selenium and high-purity arsenic with the purity of 5N, accurately weighing the high-purity germanium with the weight of 494.111g, the high-purity antimony with the weight of 354.958g and the high-purity selenium with the weight of 1150.931g by using an electronic balance, sequentially loading the two raw materials into the quartz tube along a loading port by using a funnel, assembling a vacuum quick interface at a tube port after loading is completed, transferring the quartz tube out of a glove box, quickly connecting a vacuum unit pipeline for evacuation treatment, keeping the quartz tube in a heating state when evacuating, and evacuating the quartz tube until the pressure in the quartz tube reaches 10 ℃ at 120 DEG C -3 After Pa or less, the quartz tube was sealed with oxyhydrogen flame.
Transferring the quartz tube into a swinging furnace for melting homogenization, quenching and forming glass liquid by using compressed air as a quenching medium after the preparation, wherein the quenching air pressure is 0.4MPa, transferring the quartz tube into an annealing furnace for annealing after the glass liquid is hardened and formed,
after the annealing is finished, the quartz tube is broken, the glass bar stock is taken out, corresponding detection is carried out on the bar stock, and the detection results are shown in the following table:
TABLE 2 Ge prepared by the same batch of reused quartz tubes 28 Sb 12 Se 60 Bar stock test results
Composition into Ge by using two quartz tubes processed in same batch 28 Sb 12 Se 60 The preparation of the chalcogenide glass bar stock, and the detection of the obtained bar stock according to national standard test standards shows that: the fringe degree of the two bars is A level, the impurity degree is 1 level, and the transmittance of different incident wavelengths and wave bands corresponding to the two bars is shown in the table above.
The above disclosed features are not intended to limit the scope of the disclosure, and therefore, equivalent variations to what is described in the claims of the disclosure are intended to be included within the scope of the claims of the disclosure.

Claims (8)

1. A method for recycling quartz tubes comprises the following steps:
step one, cutting off a section of residual vapor transmission pipe connected with a material containing pipe of a raw H-shaped quartz pipe after distillation purification of chalcogenide glass leftover materials at a joint part, and treating a fracture part;
step two, placing the treated quartz tube in a sodium hydroxide solution for soaking, and keeping the temperature of the alkali liquor at 80-100 ℃ in the soaking process;
taking out the quartz tube after the soaking is finished, using pure water to wash out alkali liquor attached to the surface of the quartz tube, transferring the alkali liquor to aqua regia to soak for 1-2 hours, then using the pure water to spray the outer wall of the quartz tube, then pouring two thirds of pure water into the quartz tube, shaking the bottle body for 8-10 times, then draining washing water in the bottle, and repeatedly cleaning for 3-5 times until residual water at the inner side of the bottle forms a film-shaped water film to uniformly flow down;
step four, using a pure water spray pipe body for 2-3 min, drying, and taking the pure water spray pipe body as required in the use process;
and fifthly, the quartz tube is used for melting the chalcogenide glass bar stock by the high-purity raw material.
2. The method for recycling quartz tubes according to claim 1, wherein,
in the first step, the quartz tube cutting tool is a water cutting grinding wheel;
in step one, the operation of processing the fracture is: the fracture is washed and wiped clean, and the cutting fracture is slightly burned by oxyhydrogen flame to remove burrs and cutting cracks at the fracture.
3. The method for recycling quartz tubes according to claim 1, wherein,
in the second step, the mass concentration of the sodium hydroxide is 10%.
4. The method for recycling quartz tubes according to claim 1, wherein,
in the second step, the soaking time is 2-3h.
5. The method for recycling quartz tubes according to claim 1, wherein,
in the third step, pure water is used for spraying the outer wall of the quartz tube for 3-5min.
6. The method for recycling quartz tubes according to claim 1, wherein,
in the fourth step, the drying temperature is kept at 110-120 ℃.
7. The method for recycling quartz tubes according to claim 1, wherein,
in step four, the drying time is kept between 3 and 5 hours.
8. The method for recycling quartz tubes according to claim 1, wherein,
in the fifth step, the melting method of the quartz tube for the high-purity raw material to carry out chalcogenide glass bar stock comprises the following steps:
transferring the dried quartz tube into a glove box for raw material filling, placing a charging hopper into a charging port, then carrying out batching and charging operations according to the elemental composition and the stoichiometric ratio of the chalcogenide glass, installing a vacuum quick connector on the charging port of the quartz tube after batching and charging are completed, transferring the quartz tube onto a vacuum unit for vacuumizing treatment, and when the pressure in the tube is lower than 10 -3 And (3) after Pa, sealing and sealing the quartz tube by using oxyhydrogen flame.
CN202210754496.6A 2022-06-28 2022-06-28 Method for recycling quartz tube Active CN114956605B (en)

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